Several of the additives were selected for more extensive
charge/discharge cycling in the small flow cell (electrode area
8cm2, electrolyte volume 60 cm3). The electrolyte was 1.5M
Pb(CH3SO3)2 + 0.9M CH3SO3H and, in each cycle, the battery was
charged at 20mAcm−2 for 2 h then discharged at the same current
density until the battery voltage dropped to 1.0 V. In the absence
of an additive, the battery can be cycled but the efficiency drops
with cycle number and a black powdery deposit (shown by X-ray
diffraction to be largely lead dioxide) accumulates in the electrolyte
over the first 10 cycles; eventually shorting of the electrodes occurs.
Several of the promising additives, e.g. TritonTM X 100 and sodium
ligninsulfonate,however, contain functional groups thatpotentially
could be oxidised at the lead dioxide electrode. Indeed, when batteries
with electrolytes containing such additives were cycled, the
electrolyte was observed to change colour and their effectiveness
in controlling the deposit quality decreased with cycling. The long
chain tetraalkylammonium cations appeared to be the preferred additive and later experimentsmainly used the hexadecyltrimethylammonium
cation as the additive.